CN104548973A - Preparation and catalytic regeneration of functionalized graphene oxide/polyether sulfone blended ultrafiltration membrane - Google Patents
Preparation and catalytic regeneration of functionalized graphene oxide/polyether sulfone blended ultrafiltration membrane Download PDFInfo
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- CN104548973A CN104548973A CN201410802820.2A CN201410802820A CN104548973A CN 104548973 A CN104548973 A CN 104548973A CN 201410802820 A CN201410802820 A CN 201410802820A CN 104548973 A CN104548973 A CN 104548973A
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- graphene oxide
- ultrafiltration membrane
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- functional graphene
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Abstract
The invention provides preparation and catalytic regeneration of a functionalized graphene oxide/polyether sulfone blended ultrafiltration membrane. The preparation method of the functionalized graphene oxide/polyether sulfone blended ultrafiltration membrane is characterized by comprising the following specific steps: dispersing cobaltosic oxide-loaded graphene oxide and a pore-foaming agent into an organic solvent with an ultrasonic wave; adding polyether sulfone to a dispersion liquid, and stirring and dissolving at 75-85 DEG C; standing and defoaming to obtain a casting liquid; scraping the casting liquid at room temperature when the environment humidity is 50%-55% to prepare a liquid membrane; and putting into a water bath at 10-25 DEG C, after the membrane falls off, taking out the membrane, washing, soaking, freezing and drying to obtain the functionalized graphene oxide/polyether sulfone blended ultrafiltration membrane.
Description
Technical field
The invention belongs to environment-friendly materials technical field, particularly a kind of modification of poly (ether-sulfone) ultrafiltration membrane and catalytic regeneration method thereof.
Background technology
The material preparing milipore filter is a lot, and early stage milipore filter take cellulose acetate as material.This material price is low, and filming performance is good, still has important purposes so far.Non-cellulose-acetafolic material has polysulfones, polyether sulfone, Merlon, polyvinyl chloride, polyimides, polytetrafluoroethylene (PTFE), Kynoar and polyelectrolyte etc.
Polyether sulfone (PES) is a kind of thermoplastic macromolecule material that 20 century 70s are developed, and has the performances such as good chemical stability, high temperature resistant, strong alkali-acid resistance, anti-oxidant and solvent resistant, is widely used in the aspects such as water treatment in recent years.Current polyether sulfone (PES) milipore filter realizes suitability for industrialized production.But polyether sulfone (PES) film hydrophobicity is strong, when processing aqueous based systems, the resistance of film is large, flux is little, and easily contaminated, must improve the contamination resistance of film by hydrophilic modification and reduce the power consumption of membrane process operation.
Summary of the invention
The object of the invention is to overcome that existing poly (ether-sulfone) ultrafiltration membrane hydrophily is poor, flux is low, pollute after cleaning recover inefficient problem, modification is carried out to poly (ether-sulfone) ultrafiltration membrane, a kind of preparation and catalytic regeneration method of functional graphene oxide/polyethersulfone blended ultrafiltration membrane are provided.
In order to achieve the above object, the invention provides a kind of preparation method of functional graphene oxide/polyethersulfone blended ultrafiltration membrane, it is characterized in that, concrete steps comprise: by load, the graphene oxide of cobaltosic oxide and the dispersion of pore-foaming agent ultrasonic wave are in organic solvent, polyether sulfone is added in the dispersion liquid of gained, stirring and dissolving under 75-85 DEG C of condition, standing and defoaming, obtains casting solution; In room temperature, ambient humidity is under the condition of 50-55%, is scraped by casting solution and makes liquid film, then puts into the water-bath of 10-25 DEG C, and after film separation, take out, washing, soak, freeze drying, obtains functional graphene oxide/polyethersulfone blended ultrafiltration membrane.
Preferably, in described casting solution, the mass percent concentration of the graphene oxide of load cobaltosic oxide is 0.1 ~ 2.0%, and the load capacity of cobaltosic oxide is 50%-70%.
Preferably, described organic solvent is the mixture of one or more in dimethyl formamide, dimethylacetylamide, METHYLPYRROLIDONE.
Preferably, in described casting solution, the mass percent concentration of polyether sulfone is 15% ~ 20%.
Preferably, described pore-foaming agent is polyvinylpyrrolidone, and in described casting solution, the mass percent concentration of pore-foaming agent is 2% ~ 5%.
Preferably, the time of described ultrasonic wave dispersion is 2-3h.
Preferably, the time 3-5h of described stirring and dissolving, the time of standing and defoaming is 0.5-1.5h.
Preferably, describedly casting solution is scraped to make liquid film be adopt flat membrane casting equipment to scrape to make liquid film.
Preferably, the thickness of described liquid film is 60 ~ 340 μm.
Preferably, described washing is distilled water washing, soaks for soaking in the glycerine water solution of 50vol%.
Preferably, the preparation method of described liquid film is: the temperature of scraping lamina membranacea, flat membrane casting equipment panel and casting solution of cleaning be consistent, set and scrape film thickness and knifing speed, scraping film thickness is 60 ~ 340 μm, knifing speed is 3000 ~ 5000mm/min, the casting solution prepared is poured over the one end of scraping lamina membranacea, startup knifing machine is scraped and is made liquid film.
Preferably, the thickness of described functional graphene oxide/polyethersulfone blended ultrafiltration membrane is that under 60-340 μm, 0.1MPa pressure, pure water flux is 100 ~ 700Lm
-2h
-1, rejection is 90-99%.
Present invention also offers the catalytic regeneration method of the functional graphene oxide/polyethersulfone blended ultrafiltration membrane prepared by preparation method of above-mentioned functional graphene oxide/polyethersulfone blended ultrafiltration membrane, it is characterized in that, concrete steps comprise: will run the milipore filter pure water backwash 15 ~ 20 minutes of a period of time, backwash operating pressure is 0.15 ~ 0.2MPa; Taken out by milipore filter after backwash, being dipped to concentration is in the monopersulfate salting liquid of 2 ~ 5mM, aeration agitation 10 ~ 30 minutes, obtains the functional graphene oxide/polyethersulfone blended ultrafiltration membrane regenerated.
Preferably, described monopersulfate salt is PMS.
Preferably, the described concentration that is dipped to by milipore filter is in the process of monopersulfate salting liquid of 2 ~ 5mM, and carry out aeration agitation, the time is 10 ~ 30 minutes simultaneously.
Compared with prior art, the invention has the beneficial effects as follows:
(1) present invention process is simple, and cost is low, is easy to industrialization;
(2) hydrophily of functional graphene oxide/polyethersulfone blended ultrafiltration membrane of preparing of the present invention, water flux, the more existing poly (ether-sulfone) ultrafiltration membrane of anti-fouling performance significantly strengthen;
(3) functional graphene oxide/polyethersulfone blended ultrafiltration membrane that prepared by the present invention has catalytic oxidation function, can produce the potentiometric titrations (SO with oxidisability by catalytic activation monopersulfate salting liquid
4 -), thus realize the cleaning and regeneration after film Organic Pollution.
Accompanying drawing explanation
Fig. 1 is polyether sulfone mass percentage concentration is 15wt%, and polyvinylpyrrolidone is 5%, and coagulation bath temperature is 20 DEG C, and casting solution temperature is 80 DEG C, the section structure electron-microscope scanning figure of pure PES film;
Fig. 2 for for polyether sulfone mass percentage concentration be 15wt%, polyvinylpyrrolidone is 5%, and the mass percentage concentration of the graphene oxide of load cobaltosic oxide is 2.0%, and coagulation bath temperature is 20 DEG C, casting solution temperature is 80 DEG C, the section structure electron-microscope scanning figure of composite hyperfiltration membrane;
Detailed description of the invention
Below in conjunction with specific embodiment, set forth the present invention further.Should be understood that these embodiments are only not used in for illustration of the present invention to limit the scope of the invention.In addition should be understood that those skilled in the art can make various changes or modifications the present invention, and these equivalent form of values fall within the application's appended claims limited range equally after the content of having read the present invention's instruction.
The graphene oxide adopted in following examples is obtained by Hummer oxidizing process, and concrete steps are:
(1) in the 2L beaker of drying, the concentrated sulfuric acid (115mL, 98%) and sodium nitrate (NaNO is added
3, 2.5g), cool under condition of ice bath.When the temperature of system is lower than 5 DEG C, in stirring, add crystalline flake graphite (5g), continue to stir 2.5h, to be mixed evenly after, slowly add potassium permanganate (KMnO
4, 15g), control reacting liquid temperature and be no more than 20 DEG C (by controlling mixing speed and dosing velocity interpolation).Then beaker is placed in the water bath with thermostatic control of 35 DEG C, uniform stirring (mechanical agitation).Liquid temp to be mixed rises to 35 DEG C, and after reacting 2h, adds deionized water (230mL), controls reacting liquid temperature at 98 DEG C.Continue to stir 15min, then add a large amount of deionized waters (0.7L) by reaction terminating.Add hydrogen peroxide (30%H simultaneously
2o
2, 12.5mL), at this moment solution becomes vivid yellow from brownish black.
(2) filter while hot, with watery hydrochloric acid (1: 10 volume ratio, 1L), centrifuge washing is carried out to product, and fully wash until without SO in filtrate by deionized water
4 2-(BaCl
2solution detects).Then dry in the vacuum drying oven of 60 DEG C, the graphite oxide number of finishing of acquisition is placed in drier preserves.
(3) graphite oxide powder 200mg is joined in n-hexyl alcohol (120ml), it is made to form homodisperse suspension by ultrasonic 2h, separately 1mmol cabaltous nitrate hexahydrate is dissolved in another part of n-hexyl alcohol (80ml), mix with the suspension containing graphite oxide after forming red solution, and at room temperature stirring 0.5h makes two kinds of materials mix uniformly.Then by mixture reflux heating 12h at 140 DEG C.By reaction system cool to room temperature after reaction terminates, centrifuge washing (centrifuge speed test regulates), and with ethanol cyclic washing to remove n-hexyl alcohol and foreign material wherein, the product dry for standby in the vacuum drying oven of 60 DEG C finally will obtained, is the graphene oxide (CO of load cobaltosic oxide
3o
4/ GO), the load capacity of cobaltosic oxide is 50%.
Embodiment 1
A preparation method for functional graphene oxide/polyethersulfone blended ultrafiltration membrane, concrete steps are:
By functional graphene oxide and pore-foaming agent polyvinylpyrrolidone at organic solvent N, in N-dimethylacetylamide, ultrasonic disperse 2 hours, adds polyether sulfone in the dispersion liquid of gained, is placed into 80 DEG C of constant temperature stirring and dissolving in water-bath, leave standstill deaeration in 1 hour, obtain casting solution; In casting solution, the mass percent concentration of the graphene oxide of load cobaltosic oxide is 0%, and in casting solution, the mass percent concentration of polyether sulfone is 15%, the polyvinylpyrrolidone of polyvinylpyrrolidone is 5%;
In room temperature, ambient humidity is under the condition of 50-55%, the temperature of scraping lamina membranacea, flat membrane casting equipment panel and casting solution of cleaning is consistent, sets and scrape film thickness and knifing speed, and scraping film thickness is 0.3mm, and knifing speed is 4000mm/min.The casting solution prepared is poured over the one end of scraping lamina membranacea, start knifing machine and scrape the liquid film made thickness and be about 0.3mm, put into 20 DEG C of water-bath film forming immediately, take out from water-bath after film separation, fully wash with distilled water, soak the solvent removing and remain in film, soak 24h with the glycerine water solution of 50vol% again, finally take out freeze drying in freeze drier, obtain functional graphene oxide/polyethersulfone blended ultrafiltration membrane.
Embodiment 2-7
Be similar to embodiment 1, difference is: in embodiment 2-7, in casting solution, the mass percent concentration of the graphene oxide of load cobaltosic oxide is followed successively by 0.1%, 0.3%, 0.5%, 0.7%, 1.0%, 2.0%.
Functional graphene oxide/polyethersulfone blended ultrafiltration membrane in embodiment 1-7 is measured under 0.1MPa pressure its pure water flux and BSA rejection (%), specific as follows:
The bovine serum albumin(BSA) (BSA) adopting 1g/L is pollutant, anti-fouling performance evaluation is carried out to the functional graphene oxide/polyethersulfone blended ultrafiltration membrane in embodiment 1-7, test process is: under room temperature, under 0.15MPa with distilled water to film precompressed 40min, then pressure is changed into 0.1MPa by measure pure water through volume calculate pure water flux, every 5min record is once through the volume of pure water, and experimental period is 30min; Then ultrafiltration solution is replaced by bovine serum albumin solution, record once through the volume of solution every 5min equally under 0.1MPa, Therapy lasted process is 3h; After completing, film is taken out, fully rinse to remove film surface smut with distilled water, and with distilled water backwash 15min under 0.15MPa, again measure pure water flux, the time is still 30min.
Pure water flux (the Lm of gained
-2h
-1) analog value is respectively 79.46,100.37,127.15,302.46,382.57,503.71,698.07; BSA rejection (%) analog value is respectively 83.3,92.4,93.2,95., 98.4,95.1,90.8.Result shows, in casting solution the mass percent concentration of the graphene oxide of load cobaltosic oxide be 0.7% milipore filter combination property best, ensure that quite high rejection maintenance is high-throughout simultaneously.
Measure the surface contact angle of the functional graphene oxide/polyethersulfone blended ultrafiltration membrane in embodiment 1-7 respectively, the contact angle data of gained are respectively 81.37 °, 70.33 °, 76.62 °, 62.57 °, 68.26 °, 55.12 °, 50.02 °.Result shows, the hydrophily of composite membrane than the good hydrophilic property of pure polyether sulfone (PES) milipore filter, functional graphene oxide add the hydrophily improving polyether sulfone (PES) milipore filter.
The section structure electron-microscope scanning figure of the functional graphene oxide/polyethersulfone blended ultrafiltration membrane of embodiment 1 and embodiment 7 respectively as depicted in figs. 1 and 2, as seen from the figure: along with adding of functional graphene oxide, the structure of milipore filter there occurs change, the thickness of top layer compacted zone reduces, inner tiny finger-like pore changes the large-scale finger-like path of connection into, the water flux of blend film is greatly improved, and compacted zone still keeps good intensity, ensure that the rejection of milipore filter.
Embodiment 2
The catalytic regeneration method of the functional graphene oxide/polyethersulfone blended ultrafiltration membrane prepared by the preparation method of the functional graphene oxide/polyethersulfone blended ultrafiltration membrane in embodiment 5, concrete steps are:
Get functional graphene oxide obtained in a slice embodiment 5/polyethersulfone blended ultrafiltration membrane and load ultrafiltration cup, precompressed 20min under pressure is 0.15MPa condition, tests pure water flux J under 0.1MPa
1for 382.57Lm
-2h
-1; In ultrafiltration cup, add second pond sewage carry out ultrafiltration operation, maintenance pressure is 0.1MPa, and every 5min surveys a flux data, continuous service 6h, and now milipore filter has pollution to a certain degree, at this moment uses the pure water flux of distilled water test membrane again, is designated as J
2for 141.29Lm
-2h
-1; Wipe the polluter on surface with moistening sponge, and with distilled water flushing, re-assemblied by film and carry out backwash afterwards, operating pressure is 0.15MPa, and backwashing time is 20min, then under 0.1MPa, tests pure water flux J
3for 225.58Lm
-2h
-1, the milipore filter after backwash is taken out, film is immersed the PMS solution that concentration is 3mM, 25 DEG C of aeration agitation 1h, with the pure water flux J retesting film after distilled water flushing
3' be 372.24Lm
-2h
-1; Substitute into formulae discovery flux recovery rate: WFR=[(J
3-J
2)/(J
1-J
2)] x100%, the flux recovery rate obtaining General Physics backwash is 58.96%, and the flux recovery rate of new membrane catalytic oxidation ablution is 97.2%.
Result shows, what add functional graphene oxide in milipore filter adds energy catalytic activation PMS solution, plays its catalytic oxidation function, removes or the auxiliary organic pollution removed in fenestra, improves the cleaning recovery efficiency of milipore filter.
Claims (10)
1. the preparation method of functional graphene oxide/polyethersulfone blended ultrafiltration membrane, it is characterized in that, concrete steps comprise: by load, the graphene oxide of cobaltosic oxide and the dispersion of pore-foaming agent ultrasonic wave are in organic solvent, polyether sulfone is added in the dispersion liquid of gained, stirring and dissolving under 75-85 DEG C of condition, standing and defoaming, obtains casting solution; In room temperature, ambient humidity is under the condition of 50-55%, is scraped by casting solution and makes liquid film, then puts into the water-bath of 10-25 DEG C, and after film separation, take out, washing, soak, freeze drying, obtains functional graphene oxide/polyethersulfone blended ultrafiltration membrane.
2. the preparation method of functional graphene oxide/polyethersulfone blended ultrafiltration membrane as claimed in claim 1, it is characterized in that, in described casting solution, the mass percent concentration of the graphene oxide of load cobaltosic oxide is 0.1 ~ 2.0%, and the load capacity of cobaltosic oxide is 50%-70%.
3. the preparation method of functional graphene oxide/polyethersulfone blended ultrafiltration membrane as claimed in claim 1, it is characterized in that, described organic solvent is the mixture of one or more in dimethyl formamide, dimethylacetylamide, METHYLPYRROLIDONE.
4. the preparation method of functional graphene oxide/polyethersulfone blended ultrafiltration membrane as claimed in claim 1, it is characterized in that, in described casting solution, the mass percent concentration of polyether sulfone is 15% ~ 20%.
5. the preparation method of functional graphene oxide/polyethersulfone blended ultrafiltration membrane as claimed in claim 1, it is characterized in that, described pore-foaming agent is polyvinylpyrrolidone, and in described casting solution, the mass percent concentration of pore-foaming agent is 2% ~ 5%.
6. the preparation method of functional graphene oxide/polyethersulfone blended ultrafiltration membrane as claimed in claim 1, it is characterized in that, the thickness of described liquid film is 60 ~ 340 μm.
7. the preparation method of functional graphene oxide/polyethersulfone blended ultrafiltration membrane as claimed in claim 1, it is characterized in that, the preparation method of described liquid film is: the temperature of scraping lamina membranacea, flat membrane casting equipment panel and casting solution of cleaning be consistent, set and scrape film thickness and knifing speed, scraping film thickness is 60 ~ 340 μm, knifing speed is 3000 ~ 5000mm/min, the casting solution prepared is poured over the one end of scraping lamina membranacea, and startup knifing machine is scraped and made liquid film.
8. the catalytic regeneration method of the functional graphene oxide/polyethersulfone blended ultrafiltration membrane prepared by the preparation method of the functional graphene oxide/polyethersulfone blended ultrafiltration membrane described in claim 1-7, it is characterized in that, concrete steps comprise: will run the milipore filter pure water backwash 15 ~ 20 minutes of a period of time, backwash operating pressure is 0.15 ~ 0.2MPa; Taken out by milipore filter after backwash, being dipped to concentration is in the monopersulfate salting liquid of 2 ~ 5mM, aeration agitation 10 ~ 30 minutes, obtains the functional graphene oxide/polyethersulfone blended ultrafiltration membrane regenerated.
9. the catalytic regeneration method of functional graphene oxide/polyethersulfone blended ultrafiltration membrane as claimed in claim 8, it is characterized in that, described monopersulfate salt is PMS.
10. the catalytic regeneration method of functional graphene oxide/polyethersulfone blended ultrafiltration membrane as claimed in claim 8, it is characterized in that, the described concentration that is dipped to by milipore filter is in the process of monopersulfate salting liquid of 2 ~ 5mM, and carry out aeration agitation, the time is 10 ~ 30 minutes simultaneously.
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| CN113289657A (en) * | 2021-05-21 | 2021-08-24 | 山西大学 | Preparation method and application of nitrogen-doped graphene catalytic membrane |
| CN115364679A (en) * | 2022-07-27 | 2022-11-22 | 中国地质大学（武汉） | Potassium ion selective film and preparation method thereof |
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| CN115364679A (en) * | 2022-07-27 | 2022-11-22 | 中国地质大学（武汉） | Potassium ion selective film and preparation method thereof |
| CN115364679B (en) * | 2022-07-27 | 2023-06-27 | 中国地质大学（武汉） | Potassium ion selective film and preparation method thereof |
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